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N-isopropylpentedrone (NiPP) synthesis       ~ def <def@huumeet.info> 2026-02-27
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M(NiPP HCl) = 255.78 g/mol
M(NiPP freebase) = 219.32 g/mol

M(2-bromo-valerophenone) = 241.124 g/mol
M(isopropylamine) = 59.112 g/mol

M(citric acid monohydrate) = 210.14 g/mol
M(NaHCO3) = 74.007 g/mol
M(Na2CO3) = 105.99 g/mol
M(HCl) = 36.46 g/mol
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n = 30 g / 255.78 g/mol =  0.1173 mol

 1. Add 28.3 g 2BrV with 100 mL EtOAc to a reaction flask.
 2. Add 20 g (~3 mol eq) isopropylamine dropwise with vigorous stirring while
    maintaining temperature below < 65C.
 3. Run the reaction for 6-10 hours after the addition of the last drop.
 4. Wash the reaction mixture 1x with 100 mL saturated NaHCO3 water.
 5. Acidify with 25 g of citric acid dissolved in 100 mL H2O, discarding
    non-polar layer.
 6. (Optional:) Wash the extracted aqueous phase with 70 mL of xylene.
 7. Basify with 38 g Na2CO3. Be careful with the released CO2(g) gas!
 8. Decant the top freebase layer and discard the bottom aqueous layer.
 9. Dissolve the freebase into a freezer-cold acetone (~0.3L ) and precipitate
    by acidifying with 4.3 g HCl, that is, 13 g (~14 mL) 33% HCl(aq) *or* until
    the pH reaches 5-6 or the further precipitation of NiPP HCl stops.
10. Filter & wash the product with freezer-cold acetone (two or three times).
    This is crucial even if the appearance of the product is white powder.
11. Dry the acetone-washed NiPP HCl powder in a room with a good ventilation.
12. (Optional:) Recrystallize the product (in acetone and/or IPA) to purify.
13. (Optional:) Slow evaporate (in H2O and/or EtOH) to get big chunky crystals.

Theoretical yield: 30 g NiPP HCl (100%)
Actual yield: 30-70%

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